Accessing NMR Files from the Teaching Laboratories Spectrometer for Reprocessing

Accessing NMR files from the Teaching Laboratories Spectrometer for reprocessing

Submitting samples After preparing NMR samples in the lab, these are labelled with a numbered tag and need submitting to the computer opposite the NMR room in the teaching laboratories. The tag number allows the technical staff to match the NMR tube to the submission in the computer and add this to the NMR spectrometer sample queue to be run. When samples are added to the queue on the spectrometer, the instrument assigns the samples experiment number(s).

Experiment numbering NMR files are organised first by the date they were run, then into subfolders by the experiment number. The date folders are in the format mmmdd-yyyy-teaching. The date folder corresponds to the date the samples were loaded onto the spectrometer. Usually, this is the same day the sample would have been submitted in the lab, however sometimes samples may be held back and run on a later date if there is a very large number of samples to run.

In order to find the experiment number allocated to your sample, you will need to look up the sample numbers in the NMR Google Sheet for that term. There are links to the Google Sheets on the NMR Instrument page, along with details about the NMR Service: https://www.york.ac.uk/chemistry/chem-intranet/ug- intranet/teachinglabs/facilities/instruments/nmr/

If you open up this page and select the ‘Accessing Spectra’ tab to find links to the sheets. After opening the Google sheet, you should have a document with a series of worksheets contained within it: The first sheet (Form responses 1) shows the list of experiments submitted to the NMR service, but which have not yet been loaded onto the NMR spectrometer for acquisition. All other sheets contain lists of experiments by the date on which they were submitted to the spectrometer.

Select the date that your samples were run (usually the day of submission) and locate your samples within this spreadsheet (it is usually easiest to search the sheet for your username!). You will need to note down the experiment number(s), to be able to view your NMR results. A note on numbering Each subfolder contains the acquired data from one NMR experiment. The first experiment for each NMR sample ends in 0, and subsequent experiments on the same sample will increase from this. Each new sample will then jump to end in 0 again. For example:

Experiment number Experiment 10 Proton on sample 1 11 Carbon on sample 1 20 Proton on sample 2 21 Carbon on sample 2 30 Proton on sample 3

Viewing NMR results PDFs are automatically produced when the experiment acquisition is completed. These are accessible from on campus using a web browser.

Note for off campus users If you are off campus, you will need to connect to campus before trying to access NMR files. There are a number of ways to do this. More information is available from IT Services: https://www.york.ac.uk/it-services/work-off-campus/

Opening the PDFs Having identified the date and sample numbers for your NMR files, open the following web address:

ftp://chemtl.york.ac.uk/NMR/

The page will display a list of dates, locate and open the date, then the experiment number for your sample.

You will get a view similar to the below: You then need to open the ‘pdata’ folder, followed by the ‘1’ folder within it. Inside that folder will be a PDF file named in the form:

Email_mmmdd-yyyy_exptno_1.pdf

This is the PDF file of your NMR results. You should be able to download/open this PDF file for analysis. If you have opened the right file it should have your name, email and title of the sample displayed in the top left corner.

Note about composite experiments Some experiments require two data folders to acquire the spectrum. Processed files for these will only exist in the second experiment number folder. This is most commonly carbon and DEPT-135 composite experiments.